Process for extracting oil from cotton-seed or other oleaginous material.



J. E. MILLS. PEOOEss EOE EXTEAOTINO OIL EROM COTTON SEED OR OTHER OLEAGINOUS MATERIAL.

APPLICATION FILED AUG.23, 1007.

Patented Mar. 2, 1909.

J. E. MILLS.

PROCESS FOR EXTRACTING OIL FROM COTTON SEED 0R OTHER OLEAGINOUS MATERIAL.

APPLIOATION FILED AUG.23, 1907.

91 3,7 5 1 Patented Mar. 2, 1909.

2 SHEETS-SHEET 2.

UNITED sTATEs PATENT OFFICE.

JAMESy EDWARD MILLS, OF CHAPEL HILL, NORTH CAROLINA, ASSIGNOR OF ONE-FOURTH TO H. B. BATTLE, OF MONTGOMERY, ALABAMA.

- To all whom it may concern:

rnocnss Fon Ex'rnac'rme on. FROM corren-SEED on OTHER oLEAGINoUs MATERIAL.-

Specification of Letters Patent.

Patented March 2, 1909.

Application med Aug'un 2s, 1907.. serial No. 389,910.

Be it known that I JAMES EDWARD MILLS, a citizen of the United States, residing at Chapel Hill, in the county of Orange and State of North Carolina, have invented certain new and useful Improvements in Processes for Extracting Oil from Cotton- Seed or other Oleaginous Material; and I do hereby declare the following to be a full, clear, and exact description of the invention,

such as will enable others skilled in the art to which it appertains to make and use the same.

My invention relates to av rocess for extracting cotton seed oil from t e cotton seed,

. from the cotton seed meats, or from cotton seed meal, which is left after the larger portion of the oil'has been pressed out, or extracting oil from other oleaginous seeds or material; and the objects of my invention are to produce a quick, safe, efficient and cheap process, which shall be capable of Y being used on a commercial scale, and which shall be certain in out.

action and easy to carry I attain the above objects by passing the cotton seed, its meats or meals, or. other oleaginous seeds or material, through any suitable apparatus, and compelling the same to come into intimate contact with liquid, or vaporous, carbon tetrachlorid CCL, or-both, whereb the oil from the same is taken up by the sai carbon tetrachlorid and I then suitably recover the said oil from the same, and also recover any carbon tetrachlorid that may be carried out of the apparatus by the cotton seed, its meats, or meal, or other oleagino'us seeds or material, as will be more vfully hereinafter disclosed.

In order to simpli the s ecification, I will .disclose in the fol owingI escription my process as .applied to the extraction of the hausted seed, meats or meal, and therefore practically completes the extraction of oil therefrom, all as will more fully appear hereinafter. y

Referring to the accompanyi g drawings, Fig.. 1, 1 represents a tube or compartment preferably of a circular cross section, supplied with a suitable opening and feed at 2 or the cotton seed, its meats, or meal, and With a screw shaft 3, p provided with a screw 31, the latter, rotated b any suitable power, and reaching preferably not lquite to the oplening of the tube 1 into compartment 4. 'l e compartment 4 is placed preferably in a vertical or nearly vertical position, and is also preferably circular in shape, and extends preferably some distance below the o ening of tube 1 into this compartment, as s own. In the chamber or compartment 4 is located a vertical shaft 5, rotated b any suitable power,n and carrying padd es 6. This chamber or compartment 4 1s provided at its bottom with a steam or water inlet pipe 7, and with an outlet pipe 8 for the caron tetrachlorid containing oil, said pipe leading into the settling tank 9. From this tank the carbon tetrachlorid Vand its contained oil is pumped through the pipe 10l to the still 11.. The chamber or compartment 4 is rovided at its top with a conveyer 12 winch carries the extracted seed, meats, or meal, to a suitable drying chamber 13. Any excess of carbon 'tetrachlorid carried over during the passage of the seed,'mcats, or

meal, through the conveyer 12, is drained through the perforated poi-.tion 12lof the conveyer 12 and is caught and carried to the settling tank 14. 15 is a reservoir for carbon tetrachlorid connecting with the still 11 through the pipe 16, with the condenser 17,

compartment '4 through the pipe 19, and with the settling tank 14 through vthe pipe 20. The 'drying chamber 13 connects with the coils 21 1n thecondenser 17'-through the pipe 22. All ipes are suitably provided with valves, an any suitable apparatus (not shown inthe drawings) is provided ,to pump- 106 through the pipes 18, with the chamber or the carbon tetrachlorid in the direction dethat a slightly compacted cake of meal 32' sired when gravityI is not suiiicient to cause its continuous loW. The screws 31 and conveyers 12 and shaft 5 are kept in motion by any suitable power.

In carrying out my process with this apparatus the cotton seed, its meats, or meal, is rst crushed or disintegrated to a suitable iineness by apparatus not shown in the drawing. The cotton seed, its meats, or meal, thus prepared enters the machine through the funnel tubev2 and is carried by the screw 31 through the tube 1 into compartment 4. The screw 31 ends slightly before reaching compartment 4, in order may be formed at the junction with compartment 4. Com artment 4 is iilled with carbon tetrachlori and the weight of this column forces some of the liquid through the meal in the lower portion of the tube 1. Therefore, the extraction of the oil from the cotton seed, its meats, or meal',` really commences in the tube 1. rlhe meal is advanced through the tube 1, with suflicient rapidity to revent.th'e appearance of any of the car on tetrachlorid at the opening 2. This is easily done since the carbon tetrachlorid penetrates the meal in the tube 1 only very slowly. The cotton seed, its meats, or meal, .after reaching compartment 4, at once attempts to rise to the top 'of the compartment,y since it is lighter than the liquid carbon tetrachlorid with which the compartment is filled. 'Although this meal, practically exhausted of its oil, eventually reaches the top ofthis chamber, its passage is obstructed and rendered somewhatI slow, by

the addles 6, attached at intervals to the slow y revolving shaft 5, which paddles are set at an angle to the shaft, and are of sufficient width to materially obstruct the rise' of the meal. These paddles, besides preventing the too rapid rise of the meal,` insure its intimate mixture and thorough contact with the carbon tetrachlorid, and at the same time prevent any possible clogging 'of the compartment 4, since by the inclination of the addles the meal is forced upward finally to t e top of the column.

Fresh and preferably hot carbon tetrachlorid continually enters at 19, near the top of the cylinder, or chamber 4, and carbon tetrachlorid containing the extracted oil-is continually'drawnfrom the lower end of the compartment 4, at the'pipe 8. In other words, the vpors and liquid of fresh hoi'l carbon tetrac orid continually entering the compartment at 19, and -meeting rst the meal, which in its tetrachlorid be ow has alrea y been largely exhausted of its oil, com letes the extraction of the oil from the mea about to leave the apparatus. Said meal, deprived of its oil, is continually removed from the top of chamber Thereby assage throu h the carbon 4, by the conveyer 12, receiving its power` compartment 4 compels the downwardilow.

Second, the density of the successive layers of the carbon tetrachlorid and its contained oil increases as it passes from the top of column 4 to the bottom, and thereby upward currents of the liquid are prevented. lThis is accomplished, in spite of the fact that the contained oil decreases the density of the carbon tetrachlorid, by causing the carbon tetrachlorid to become cooler as it descends.

tetrach oridv as -it descends and becomes richer in oil, is balanced, vor more than' therefore the latter would show an aggravat ing tendency to rise to the top of chamber 4, which tendency could only be overcome, if at all, by an increased rapidity of circulation of the carbon tetrachlorid, and this would materially increase the cost of the operation.

The carbon tetrachlorid and its contained oil, is asy above. stated, drawn off from the bottom of com artment 4, through the pipe 8 into the sett ing tank 9.. That portion of` compartment 4, below the entrance of tube 1, itself serves as a settling tank and only 'the iinest silt and residue from the meal linally finds its way into the settling tank 9, from the top of which it is remove'd and agaln caused to enter the machine at 2. The carbon tetrachlorid containing the dissolved oil is 'removed from the bottom of the tank 9 to the still 11 where it is distilled from the oil, under diminished pressure when advantageous, and the condensed carbon tetrachlorid and some vapor is caused to enter the top of compartment 4 hot. This'may be effected by any suitable arrangementwhatever, but

in the a paratus shown in the drawing is eflected y causing the vapors from the still 11 topass to the bottom of the reservoir 15,

where they are partially condensed as they pass through the ,contained carbon tetrachlorid, keeping it hot. Some of the un- 4condensed vapors' pass directly through the the decrease in density of the carbon the useful pur ose of further heating the finally returned to the reservoir 15.y

meal and car )on tetrachlorid contained therein. The remainder of the uncondensed vapor-of the carbon tetrachlorid passes into the condenser 17 where it is condensed and returned to the reservoir 15. 'lhe oil, still containing some carbon tetrachlorid, is removed from the bottom of the still 11 to other apparatus, not shown, for final purification. In this apparatus may be provided the usual means for agitating the oil, and also for'blowing a current of air or steam over the oil, thereby carryinvaway the vapors of the carbon tetrachlorid to be condensed and The carbon, tetrachlorid is. removed `from the extracted meal in any suitable drying'or separatin apparatus 13, the details of which are not s own since they must vary depending on whether water is used at the top of chamwith the conveyer K delivering ycompartment G, as illustrated.

'R at any convenient point.

berA or not. The carbon tetrachlorid vapors removed from the meal in this drying or separating apparatus are also condensed and returned to the reservoir 15, nally to enter the 4column 4 again.

This same process may also be carried out in the apparatus shown in Fig. 2, wherein A represents a central chamber or compartment, and B and W represent adjoining chambers or compartments. Between the chambers A and B and W are small passages F and D, formed by perforating the walls of the chamber A. G represents a third chambe-rpreferably circular in cross section and located to one side of the chamber B. In the chamber or compartment G, is located a vertical shaft H, rotated by an suitable power, and carrying paddles I. -he shaft, at its bottom, 1s provided with the large paddles J and the compartment at its to is provided into thp tank or separator L, as shown. l?l`he compartment G is enlarged at its bottom, as shown, and is provided Iwith a steam or water pipe M, and the compartment B is provided with a ste-am pipe N at its bottom, and also with an outlet pipe 0., for the c-arbon tetrachlorid,

'as shown. All of these pipes are provid-ed with valves, and' the pipe-O leads into the still, or other separating apparatus P. From this still, the i e Q leads to and extends to the ybottom oiptiie Lacket R, surrounding the upper end of chamer A, as shown, and from this jacket R, leads the pipe S, which delivers into theupper end of the chambe-r oir` A i e .connects the separator L with the saidli zibket In carrying out my aprocess with this apparatus, I cause the me to .enter at the top ofchamber, or compertinent A. This compartment contains bon tetrachlorid to the bottom of said chamber; for, although the liquid carbon tetrachlorid is very heavy, and a small amount of the meal will float on the surface of the same, yet, as the meal continually enters the chamber, the weight ofthe descending meal forces the previously floating meal, finally, to the bottom of the compartment, from where it is continually removed by the puddles J, attzu-luul to the revolvingshaft ll. These paddles eventuallybring the meal to the bottom of the elm|nbdr(l,'whieh also con-- tains carbon tetl-'achlorid and may contain a layer of water at the top, not shown, and since the meal is lighter than thel carbon tetrachlorid it tends to rise to the surface ci the same in the said chamber G, but practically exhausted of its oil. Although this meal eventually reaches the to of this chamber, its passage is obstructed) and rendered sonuswhat slow, by the addles I, at-' tached at intervals to the shaft l, which paddles are set at an` angle to the shaft, and are of sufficient width to materially obstruct thel rise of the meal. y

Fresh and hot carbon tetraehlorid continually enters at C, nearthe top of the cylinder, or chamber G, and carbon tetrachlorid containing the extracted oil is continually drawn from the com art-ment B. 1n other words, the vapors alu liquid of fresh hot earbon tetrachlorid continually enteringl the com artment at C, and meeting first the mea which in itspassage through the carbon Atetrachlorid below, has already beenlargely exhausted of its oil, com letes the extraction of the oil from the mea about to leave the apparatus. Said meal is made to pass by means of any suitable conveyer, as

-that shown, through the water supported at the top of said chamber should said water be present, and thel carbon tctrachlorid is driven from the meal partly by the mechanical action of the water, through the 'fact that the water is kept hot and therefore vaporizes the carbon tetrachlorid. The vapo- .rized carbon tetrachlorid isl of course later condensed and recovered, and the water is afterward passed from the meal, or the meal may be simply delivered into the separator L, where the carbon tetrachlorid contained in the meal is separated out by any suitable means'and returned through the pipe 'l" to the jacket R, and finally'to the meal in chamber G.

The Water at the topv of chamber (l may be introduced either as such, or as steam.

The water o'r steam may be caused to enter the chamber G through the pipe M, situated where most desirable, but shown in the drawing as near 'the bottom of chamber G. The steam condensing in its passage through the carbon tetrachlorid and meal, heats them, and at the same tune produces a more rapid rise of the meal t'owar( the top Avolved are identical.

of the chamber G. The resence of Water appears slightly to aid t e extraction. A layer of water may also be kept at the top of compartments B and W in order to prevent the evaporation of the carbon tetrachlorid.

In each apparatus the operation is sbstautially the same, and the principles in- In the machine shown in Fig. 2, however, as well as in the machine shown in Fig. l, the meal or meats do not take any longer than five minutes to complete the circulation through the various compartments, and each apparatus is designed to handle six tons of meal in ten hours, the meal entering each machine' at the rate of about twenty pounds per minute.

Referring more particularly to -the machine sho'a n in Fig. 2, the fresh carbon tetrachlorid, more or less charged with cotton seed oil, after'having., passed through chamber G, passes on into chamber, or compartment B, either very slowly through the meal at the bottom of chamber A, because the meal is there compressed by the weightof the meal above it, or it passes more ra idly by going through the ne openings in the wall of compartment G, and thence through the other openings D across` the meal in compartment A, where the meal is less compressed than at the bottom, and

finally it passes into the compartment B, as

shown bythe arrows, having/,become well The saturated `with oil in the mean time.

carbon tetrachlorid and its contained oil is as above stated, next drawn off from the compartment B, Vand led to a suitablel still P, Where the carbon tetrachlorid is separated from the oil, and returned in a hot and more or less vaporous state to chamber G. The heat given out during the condensation of the vapor, when desirable, is made use of to heat the descending meal .by circulating the said vapors around the entering meal in the jacket R at the top of chamber A, as shown, but not sufficient heat is withdrawn in this manner, to prevent the vapors and liquid entering chamber G hot, since in this condition they best extract substantially all the oil from the nearly exhausted meal.

The rapidity lwith which the carbon tetrachlorid containing oil should be drawn from compartment 4, or B, and the amount of oil which such carbon tetrachlorid should contain, will depend largely o n the amount of oil in the meal or in the meats used. 'The rule to be followed should be that the carbon tetrachlorid drawn off should contain at least as large a percentage of oil by weight as that left contained in the incoming meal,

provided that this percentage of oil in the carbon tetrachlorid does not so alter its specific gravity as to aggravate the tendency of the more saturated carbon tetrachlorid to rise to the top of chambers 4, and Grv as hereinbefore alluded to and explained. It is obvious that any? other equivalent solvent having a specific gravity greater than the exhausted meal or meats of the oleaginous material operated upon might be used instead of carbon tetrachlorid without departing from the spirit of my invention. ,v

I do not desire to be understood as limiting myself to the exact details of the process herein disclosed, for it is evident that the same could be varied by those skilled in the art without departing from the spirit of my invention.

What I claim is `1. The process of extracting oil from oleaginous material, which consists in passing carbon tetrachlorid downward, at any suitable temperature, through a suitable column; introducingA said material into said column a considerable distance below the top thereof, to cause by the buoyancy of the said material in the carbon tetrachlorid the passage of the same through the said column, and in an upward direction; and finally recovering the extracted oil from the said carbon tetrachlorid, substantially as described.

2.'The continuous process of extracting oil from oleaginous material, which consists in passing carbon tetrachlorid, at any suitable temperature, downward through a suitable column by the action of gravity, and simul- -with water near the top of said carbon tetrachlorid; and nally recovering the oil from the carbon tetrachlorid, substantially as described.

3. The process of extracting oil from oleaginous material and recovering the solvent, which consists in passing carbon tetrachlorid at any suitable temperature downward into a suitable column introducing said material into said column a considerable distance below the to thereof, to cause by the combined action o gravity and the buoyancy of the oleaginous material in the said carbon tetrachlorid the passage of the material to the top of the said column; simul^ taneously permittin the said carbon tetrachlorid to dissolve t e oil in the oleaginous `material; and removingA said olea inous materia-l more or less exhausted of its oil from the top of said column; then drawing offthe carbon tetrachlorid and its centaine oil from the bottom of said column and recovering the said carbon ^tetrachlorid from Athe contained oil, substantially as described.

. 4. The process of extracting oil from.

oleaginous seed material which consists in passing carbon tetrachlorid in' a certain rection, through a suitable apparatus, and in l in a certain direction, and simultaneously passing the constituents of sald seed through said a aratus in contact with said carbon tetrac orid and in a direction opposite to that of the latter, whereby the practically exhausted seed material is subjected to the action of the fresh carbon tetrachlorid, allowing the densities of the successive layers of said carbon tetrachlorid and its contained oil to increase as it passes through said apparatus, and ermitting the action of gravity on said ayers to prevent upward currents in the liquid, then withdrawing the carbon. tetrachlorid containing the oil, and finally separating the oil from the same, substantially as described.

5. The process of extracting oil from cotton seed material, whichconsists in passing hot carbon tetrachlorid, in a certain direcf tion through a suitable apparatus, and simultaneously passing the said seed material through the same in an opposite direction and in intimate contact with the carbon tetrachlorid, whereby the practically exhausted seed material is subjected to the action of the fresh and hot carbon tetrachlorid, allowing the densities of the successive layers ofsaid carbon tetrachlorid and its contained oil to increase as it passes through said apparatus, and permitting the action of gravity on said layers to prevent upward currents in the liquid, then withdrawing the oil and carbon tetrachlorid into a suitable still and there separating the same, and iinally returning the recovered carbon tetrachlorid to said apparatus, substantially as described. y

6. The process of extracting oil from cotton seed material, which consists in passing the same through a suitable apparatus in a certain direction and simultaneously passing carbon tetrachlorid through the same in an opposite direction, said carbon tetrachlorid being in a fresh, hot, and more or less vaporous state when it enters the apparatus and contacts with the practically exhausted seed material, allowing the densities of the successive layers of said carbon tetrachlorid and its contained oil to increase as it passes through said apparatus, and permitting the action of gravity on said layers to prevent upward currents in the liquid, then withdrawing the oil and carbon tetrachlorid, to a suitable still and separatin the one from the other, then returning the ot carbon tet-rachlorid to a suitable condenser, and extracting a portion of its heat therefrom, and finally passing said recovered and more or less vaporous carbon tetrachlorid again through the a aratus, substantially as described.

7. llie continuous process of extracting oil from cotton seed material, and recovering the solvent, which consists in continuously passing carbon tetrachlorid at any suitable temperature througha suitable apparatus passing the said seed material, through the same in an opposite direction, and through a layer of water on top of said carbon tetrachlorid, allowing the densities of the successive layers of said carbon tetrachlorid and its contained oil to increase as it passes through said apparatus, and permitting the action of gravity on said layers to prevent upward currents in the liquid, then continuously removing the exhausted seed material, from the apparatus to a suitable separator, and there separating out any carbon tetrachlorid that may be contained in the seed material, and also continuously removing the carbon tetrachlorid containing the oil to a suitable still and there separating the same from said oil, and finally returning the recovered carbon tetrachlorid to the apparatus, substantially as described.

8. `The continuous process of extracting oilfrom cotton seed material, which consists in passing carbon tetrachlorid at any suitable temperature through a suitable apparatus and in a certain direction by the action of gravity, and simultaneously passing the said seed material, through the same and in an opposite direction by the combined action of gravity and the buoyancy of the seed material, in the carbon tetrachlorid, allowin the densities of the successive layers of sai carbon tetrachlorid and its contained oil to increase as it passes through said apparatus, and permitting the action of gravity on said layers to revent upward currents in the liquid, and) finally recovering the oil from the carbon tetrachlorid, substantially as described.

9. The continuous process of extracting oil from cotton seed material, which consists in continuously passing carbon tetrachlorid at any suitable temperature through a suitable a paratus under the action of gravity, an simultaneously passing the said seed material in an o posite direction through said apparatus un er the combined action of gravity and buoyancy of said seedmaterial, and through a layer of water; allowing the densities of the successivelayers of said carbon tetrachlorid and its contained oil to increase as it passes through said apparatus, and permitting the action of gravity on said la ers to prevent upward currents in the liquid, and fnallyrecovering the oil thus extracted, substantially as described.

10. The continuous process of extracting oil from oleaginous materials, which consists in passing hot carbon tetrachlorid through a suitable apparatus in a given direction, simultaneously passing said materials through said apparatus in an opposite direction and in intimate contact with said carbon tetrachlorid, thereby successively increasing the quantity of oil absorbed, and

successively .lessening the `density lof the mixed o il and solvent, retarding the natural tendency of said ,materials to rise in the solvent; allowing the mixed oil vand solvent to cool, and allowing the increased density of the same due to said cooling, 'to overcome the said decreased density oi' the mixture due to said increased quantities of oil absorbed, and thereby causing the said cooling t0 automatically aid in the circulation of the said mixture through the machine, under the action of gravity, substantial-ly as described.

, 11. Thel process of' extracting oil from cotton seed material, .and recovering the solvent, which consists in iassing carbon tetrachlorid at any suitable temperature into a suitable chamber or compartment, causing it to come into contact with said material, permitting the said carbon tetrachlorid to cool, and by the combined wcon- {sequent increase in density, the action of l gravity and the buoyancy of the said material in the said carbon ,tetraclilorid permittingthe same to'be carried to the bottom of the said chamber orcompartment, vsimultaneously permitting the said carbon tetrachlorid to disssolve the oil in the oleaginous material, and simultaneously nous material to rise to the top of said compartment, then drawing ol the carbon tetrachloridand its contained oil from lthe bottom of the said compartment and recovering the said carbon tetrachlorid iromthe dissolved oil, substantially as described.

In ltestimony whereof, I a'iix my signature in presence of two witnesses.

JAMES EDWA {I} MILliS. l/Vitnesses:

GEO. B. Pi'rrs, L. C. BRADY.

permitting the more or less extracted 01eag1-. 

